CN105368330A - Alpha-cyanoacrylate heat-conducting glue and preparation method thereof - Google Patents
Alpha-cyanoacrylate heat-conducting glue and preparation method thereof Download PDFInfo
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- CN105368330A CN105368330A CN201510815239.9A CN201510815239A CN105368330A CN 105368330 A CN105368330 A CN 105368330A CN 201510815239 A CN201510815239 A CN 201510815239A CN 105368330 A CN105368330 A CN 105368330A
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- IJVRPNIWWODHHA-UHFFFAOYSA-N 2-cyanoprop-2-enoic acid Chemical compound OC(=O)C(=C)C#N IJVRPNIWWODHHA-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000003292 glue Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- MHJAJDCZWVHCPF-UHFFFAOYSA-L dimagnesium phosphate Chemical compound [Mg+2].OP([O-])([O-])=O MHJAJDCZWVHCPF-UHFFFAOYSA-L 0.000 claims abstract description 61
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000000049 pigment Substances 0.000 claims abstract description 21
- 229920002367 Polyisobutene Polymers 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 239000003063 flame retardant Substances 0.000 claims abstract description 7
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinyl group Chemical group C1(O)=CC(O)=CC=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 239000012153 distilled water Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical group [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 15
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 15
- 239000000975 dye Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 238000001125 extrusion Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 8
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- 239000011231 conductive filler Substances 0.000 claims description 7
- 239000004902 Softening Agent Substances 0.000 claims description 6
- 230000008719 thickening Effects 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 abstract description 3
- 239000003431 cross linking reagent Substances 0.000 abstract 1
- 229910000395 dimagnesium phosphate Inorganic materials 0.000 abstract 1
- 239000003112 inhibitor Substances 0.000 abstract 1
- 239000004014 plasticizer Substances 0.000 abstract 1
- 239000003381 stabilizer Substances 0.000 abstract 1
- 239000002562 thickening agent Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 13
- 239000011159 matrix material Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZMARGGQEAJXRFP-UHFFFAOYSA-N 1-hydroxypropan-2-yl 2-methylprop-2-enoate Chemical compound OCC(C)OC(=O)C(C)=C ZMARGGQEAJXRFP-UHFFFAOYSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 1
- 101100387911 Caenorhabditis elegans dop-2 gene Proteins 0.000 description 1
- 101100387915 Caenorhabditis elegans dop-4 gene Proteins 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- -1 acrylic ester Chemical class 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 101150097115 dop-3 gene Proteins 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000009462 micro packaging Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
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- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides alpha-cyanoacrylate heat-conducting glue. The alpha-cyanoacrylate heat-conducting glue comprises the following components in parts by weight: 100 parts of alpha-cyanoacrylate, 2-5 parts of a thickening agent, 2-4 parts of a plasticizer, 0.1-0.4 parts of a stabilizing agent, 0.5-1 part of a polymerization inhibitor, 20-30 parts of a cross-linking agent, 3-6 parts of a fire retardant, 1-2 parts of pigment, 100-110 parts of a heat-conducting filling material, 10-14 parts of magnesium hydrogen phosphate, and 8-10 parts of liquid polyisobutylene. The invention also provides a preparation method of the alpha-cyanoacrylate heat-conducting glue. The alpha-cyanoacrylate heat-conducting glue has good impact-resistance performance and heat-resistance performance.
Description
Technical field:
The present invention relates to a kind of heat-conducting glue, particularly relate to a kind of α-cyanoacrylate heat-conducting glue and preparation method thereof.
Background technology:
Heat-conducting glue; refer to for encapsulating the sizing agent with the heat conduction of heat interfacial material; be used for the bonding of electrical insulating property occasion; the bonding of such as transistor and scatterer; the protection of tube core, the sealing of shell, the heat conductive insulating of rectifier, thermistor; multiple-plate heat conductive insulating assembling in micro-packaging, chemical industry heat exchanger bonding and heat conduction embedding etc.Heat-conducting glue is generally made up of resin matrix, heat conductive filler and auxiliary agent that cohesive strength is higher, and the resin matrix of heat-conducting glue generally comprises several classes such as epoxy resin, silicone resin, acrylate resin, urethane.Wherein, acrylate resin generally adopts α-cyanoacrylate, and its advantage comprises: the cyano group 1) containing strong polarity and ester bond, therefore has very high cohesive strength to polarity adherend; 2) do not need separately to add solidifying agent, by absorbing the moisture in air or on adherend surface, anionoid polymerization occurs and realizes solidification, thus curing speed is exceedingly fast, and namely gluing rear 10-30s has enough intensity; 3) coating performance is better, easily moistening with infiltration, does not need heating or pressurization, presses, easy to use; 4) oil-proofness and resistance to air loss stronger.But, also there is certain defect in α-cyanoacrylate heat-conducting glue: impact resistance and thermotolerance poor, limit its range of application.
Publication number is CN103484052B, publication date is 2014.12.31, application people is that the Chinese patent application of Dongguan You Bang material Science and Technology Ltd. discloses " a kind of fix and the acrylic ester adhesive of heat conductive flame-retarding for heating element and heat dissipation metal chip architecture ", and it is made up of the raw material of following mass parts: the aluminium hydroxide of the prepolymer of 13-15 part, the Rocryl 410 of 9-12 part, 0-73.5 part, the aluminum oxide of 0-13.5 part, the dicumyl peroxide of 0.4-0.6 part, the white carbon black of 0.1-0.3 part, the glass microsphere of 0.5-1 part.The glue paste excellent property that this invention provides, can solve deficiency and the fast setting problem of Heating element and radiator element machine riveting, and easy to use.But there is impact resistance and the poor problem of thermotolerance equally in this acrylate adhesive.
Summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of α-cyanoacrylate heat-conducting glue, and it has good impact resistance and thermotolerance simultaneously.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of α-cyanoacrylate heat-conducting glue, by weight, is made up of following component: α-cyanoacrylate 100 parts, thickening material 2 ~ 5 parts, 2 ~ 4 parts, softening agent, stablizer 0.1 ~ 0.4 part, stopper 0.5 ~ 1 part, linking agent 20 ~ 30 parts, fire retardant 3 ~ 6 parts, pigment 1 ~ 2 part, heat conductive filler 100 ~ 110 parts, secondary magnesium phosphate 10 ~ 14 parts, liquid polyisobutene 8 ~ 10 parts.
Preferably, thickening material of the present invention is PMMA.
Preferably, softening agent of the present invention is DOP.
Preferably, stablizer of the present invention is sulfurous gas.
Preferably, stopper of the present invention is Resorcinol.
Preferably, linking agent of the present invention is cyanacrylate.
Preferably, fire retardant of the present invention is aluminium hydroxide.
Preferably, pigment of the present invention is pigment dyestuff.
Preferably, heat conductive filler of the present invention is aluminum oxide or silica powder.
Another technical problem that the present invention will solve is to provide the preparation method of above-mentioned α-cyanoacrylate heat-conducting glue.
For solving the problems of the technologies described above, technical scheme is:
A preparation method for α-cyanoacrylate heat-conducting glue, its step is as follows:
(1) secondary magnesium phosphate is added be uniformly dispersed in distilled water after obtain the secondary magnesium phosphate solution that massfraction is 10%, be that the octadecyl trimethyl ammonium chloride of secondary magnesium phosphate 1.8 times adds in secondary magnesium phosphate solution by weight, magnetic agitation 3 hours after microwave heating to 90 DEG C, dehydrated alcohol suction filtration is used after taking out, with distilled water wash 5 times, dry 4 hours at being placed in 90 DEG C, baking oven, after grinding, obtain the secondary magnesium phosphate that organises;
(2) secondary magnesium phosphate that organises that α-cyanoacrylate and step (1) obtain is added in kneader and mediate 3 hours at 130 DEG C, be transferred in twin screw extruder and melt extrude 9 minutes, extrusion temperature is 170-210 DEG C, obtains base-material after cooling;
(3) base-material that step (2) obtains is added in stirring tank, stir and add fire retardant, pigment, heat conductive filler, liquid polyisobutene after 10 minutes, stir 2 hours at 100 DEG C, add thickening material after being cooled to room temperature, softening agent, stablizer, stopper, linking agent be stirred to and be uniformly dispersed, obtain α-cyanoacrylate heat-conducting glue.
Therefore compared with prior art, the present invention has following beneficial effect:
1) secondary magnesium phosphate is a kind of inorganic materials with laminate structure, its resistance to elevated temperatures is better than α-cyanoacrylate matrix, after the organic modification of octadecyl trimethyl ammonium chloride (hereinafter referred to as 183), the molecular chain of 183 expands the interlamellar spacing of secondary magnesium phosphate, microwave heating also promotes the increasing of interlamellar spacing, after α-cyanoacrylate matrix melt blending, the molecule of α-cyanoacrylate is inserted into the interlayer of secondary magnesium phosphate, define the intercalated compound that intercalation rate is higher, when heat-conducting glue is in hot environment, the α-cyanoacrylate matrix of secondary magnesium phosphate to interlayer that resistance to elevated temperatures is stronger can play heat protective effect, can α-cyanoacrylate be effectively avoided to be subject to high temperature, thus greatly improve heat decomposition temperature and the thermotolerance of heat-conducting glue.
2) liquid polyisobutene is through just from the obtained polymkeric substance of polymerization by iso-butylene, there is good elasticity, when heat-conducting glue is subject to external impact effect, the good liquid polyisobutene of elasticity can preferentially carry consumption impact energy, greatly reduce the impact fracture that α-cyanoacrylate matrix is subject to, thus effectively improve the impact resistance of heat-conducting glue.
Embodiment:
Describe the present invention in detail below in conjunction with specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment 1
α-cyanoacrylate heat-conducting glue, by weight, is made up of following component: α-cyanoacrylate 100 parts, PMMA3 part, DOP2 part, sulfurous gas 0.1 part, Resorcinol 1 part, cyanacrylate 25 parts, 3.5 parts, aluminium hydroxide, pigment dyestuff 1.2 parts, silica powder 104 parts, secondary magnesium phosphate 13 parts, liquid polyisobutene 8.5 parts.
The step of its preparation method is as follows:
(1) secondary magnesium phosphate is added be uniformly dispersed in distilled water after obtain the secondary magnesium phosphate solution that massfraction is 10%, be that the octadecyl trimethyl ammonium chloride of secondary magnesium phosphate 1.8 times adds in secondary magnesium phosphate solution by weight, magnetic agitation 3 hours after microwave heating to 90 DEG C, dehydrated alcohol suction filtration is used after taking out, with distilled water wash 5 times, dry 4 hours at being placed in 90 DEG C, baking oven, after grinding, obtain the secondary magnesium phosphate that organises;
(2) secondary magnesium phosphate that organises that α-cyanoacrylate and step (1) obtain is added in kneader and mediate 3 hours at 130 DEG C, be transferred in twin screw extruder and melt extrude 9 minutes, extrusion temperature is 170-210 DEG C, obtains base-material after cooling;
(3) base-material that step (2) obtains is added in stirring tank, stir and add aluminium hydroxide, pigment dyestuff, silica powder, liquid polyisobutene after 10 minutes, stir 2 hours at 100 DEG C, add PMMA, DOP after being cooled to room temperature, sulfurous gas, Resorcinol, cyanacrylate be stirred to and be uniformly dispersed, obtain α-cyanoacrylate heat-conducting glue.
Embodiment 2
α-cyanoacrylate heat-conducting glue, by weight, is made up of following component: α-cyanoacrylate 100 parts, PMMA2 part, DOP4 part, sulfurous gas 0.4 part, Resorcinol 0.7 part, cyanacrylate 27 parts, 4 parts, aluminium hydroxide, pigment dyestuff 1.4 parts, 108 parts, aluminum oxide, secondary magnesium phosphate 14 parts, liquid polyisobutene 8.8 parts.
The step of its preparation method is as follows:
(1) secondary magnesium phosphate is added be uniformly dispersed in distilled water after obtain the secondary magnesium phosphate solution that massfraction is 10%, be that the octadecyl trimethyl ammonium chloride of secondary magnesium phosphate 1.8 times adds in secondary magnesium phosphate solution by weight, magnetic agitation 3 hours after microwave heating to 90 DEG C, dehydrated alcohol suction filtration is used after taking out, with distilled water wash 5 times, dry 4 hours at being placed in 90 DEG C, baking oven, after grinding, obtain the secondary magnesium phosphate that organises;
(2) secondary magnesium phosphate that organises that α-cyanoacrylate and step (1) obtain is added in kneader and mediate 3 hours at 130 DEG C, be transferred in twin screw extruder and melt extrude 9 minutes, extrusion temperature is 170-210 DEG C, obtains base-material after cooling;
(3) base-material that step (2) obtains is added in stirring tank, stir and add aluminium hydroxide, pigment dyestuff, aluminum oxide, liquid polyisobutene after 10 minutes, stir 2 hours at 100 DEG C, add PMMA, DOP after being cooled to room temperature, sulfurous gas, Resorcinol, cyanacrylate be stirred to and be uniformly dispersed, obtain α-cyanoacrylate heat-conducting glue.
Embodiment 3
α-cyanoacrylate heat-conducting glue, by weight, is made up of following component: α-cyanoacrylate 100 parts, PMMA4 part, DOP2.5 part, sulfurous gas 0.2 part, Resorcinol 0.5 part, cyanacrylate 20 parts, 6 parts, aluminium hydroxide, pigment dyestuff 1.5 parts, 105 parts, aluminum oxide, secondary magnesium phosphate 12.5 parts, liquid polyisobutene 9 parts.
The step of its preparation method is as follows:
(1) secondary magnesium phosphate is added be uniformly dispersed in distilled water after obtain the secondary magnesium phosphate solution that massfraction is 10%, be that the octadecyl trimethyl ammonium chloride of secondary magnesium phosphate 1.8 times adds in secondary magnesium phosphate solution by weight, magnetic agitation 3 hours after microwave heating to 90 DEG C, dehydrated alcohol suction filtration is used after taking out, with distilled water wash 5 times, dry 4 hours at being placed in 90 DEG C, baking oven, after grinding, obtain the secondary magnesium phosphate that organises;
(2) secondary magnesium phosphate that organises that α-cyanoacrylate and step (1) obtain is added in kneader and mediate 3 hours at 130 DEG C, be transferred in twin screw extruder and melt extrude 9 minutes, extrusion temperature is 170-210 DEG C, obtains base-material after cooling;
(3) base-material that step (2) obtains is added in stirring tank, stir and add aluminium hydroxide, pigment dyestuff, aluminum oxide, liquid polyisobutene after 10 minutes, stir 2 hours at 100 DEG C, add PMMA, DOP after being cooled to room temperature, sulfurous gas, Resorcinol, cyanacrylate be stirred to and be uniformly dispersed, obtain α-cyanoacrylate heat-conducting glue.
Embodiment 4
α-cyanoacrylate heat-conducting glue, by weight, is made up of following component: α-cyanoacrylate 100 parts, PMMA2.5 part, DOP3.5 part, sulfurous gas 0.4 part, Resorcinol 0.8 part, cyanacrylate 30 parts, 3 parts, aluminium hydroxide, pigment dyestuff 2 parts, silica powder 106 parts, secondary magnesium phosphate 12 parts, liquid polyisobutene 9.5 parts.
The step of its preparation method is as follows:
(1) secondary magnesium phosphate is added be uniformly dispersed in distilled water after obtain the secondary magnesium phosphate solution that massfraction is 10%, be that the octadecyl trimethyl ammonium chloride of secondary magnesium phosphate 1.8 times adds in secondary magnesium phosphate solution by weight, magnetic agitation 3 hours after microwave heating to 90 DEG C, dehydrated alcohol suction filtration is used after taking out, with distilled water wash 5 times, dry 4 hours at being placed in 90 DEG C, baking oven, after grinding, obtain the secondary magnesium phosphate that organises;
(2) secondary magnesium phosphate that organises that α-cyanoacrylate and step (1) obtain is added in kneader and mediate 3 hours at 130 DEG C, be transferred in twin screw extruder and melt extrude 9 minutes, extrusion temperature is 170-210 DEG C, obtains base-material after cooling;
(3) base-material that step (2) obtains is added in stirring tank, stir and add aluminium hydroxide, pigment dyestuff, silica powder, liquid polyisobutene after 10 minutes, stir 2 hours at 100 DEG C, add PMMA, DOP after being cooled to room temperature, sulfurous gas, Resorcinol, cyanacrylate be stirred to and be uniformly dispersed, obtain α-cyanoacrylate heat-conducting glue.
Embodiment 5
α-cyanoacrylate heat-conducting glue, by weight, is made up of following component: α-cyanoacrylate 100 parts, PMMA4.5 part, DOP3 part, sulfurous gas 0.3 part, Resorcinol 0.6 part, cyanacrylate 28 parts, 5.5 parts, aluminium hydroxide, pigment dyestuff 1 part, 110 parts, aluminum oxide, secondary magnesium phosphate 10 parts, liquid polyisobutene 8 parts.
The step of its preparation method is as follows:
(1) secondary magnesium phosphate is added be uniformly dispersed in distilled water after obtain the secondary magnesium phosphate solution that massfraction is 10%, be that the octadecyl trimethyl ammonium chloride of secondary magnesium phosphate 1.8 times adds in secondary magnesium phosphate solution by weight, magnetic agitation 3 hours after microwave heating to 90 DEG C, dehydrated alcohol suction filtration is used after taking out, with distilled water wash 5 times, dry 4 hours at being placed in 90 DEG C, baking oven, after grinding, obtain the secondary magnesium phosphate that organises;
(2) secondary magnesium phosphate that organises that α-cyanoacrylate and step (1) obtain is added in kneader and mediate 3 hours at 130 DEG C, be transferred in twin screw extruder and melt extrude 9 minutes, extrusion temperature is 170-210 DEG C, obtains base-material after cooling;
(3) base-material that step (2) obtains is added in stirring tank, stir and add aluminium hydroxide, pigment dyestuff, aluminum oxide, liquid polyisobutene after 10 minutes, stir 2 hours at 100 DEG C, add PMMA, DOP after being cooled to room temperature, sulfurous gas, Resorcinol, cyanacrylate be stirred to and be uniformly dispersed, obtain α-cyanoacrylate heat-conducting glue.
Embodiment 6
α-cyanoacrylate heat-conducting glue, by weight, is made up of following component: α-cyanoacrylate 100 parts, PMMA5 part, DOP2.4 part, sulfurous gas 0.1 part, Resorcinol 0.9 part, cyanacrylate 24 parts, 5 parts, aluminium hydroxide, pigment dyestuff 1.6 parts, silica powder 100 parts, secondary magnesium phosphate 11 parts, liquid polyisobutene 10 parts.
The step of its preparation method is as follows:
(1) secondary magnesium phosphate is added be uniformly dispersed in distilled water after obtain the secondary magnesium phosphate solution that massfraction is 10%, be that the octadecyl trimethyl ammonium chloride of secondary magnesium phosphate 1.8 times adds in secondary magnesium phosphate solution by weight, magnetic agitation 3 hours after microwave heating to 90 DEG C, dehydrated alcohol suction filtration is used after taking out, with distilled water wash 5 times, dry 4 hours at being placed in 90 DEG C, baking oven, after grinding, obtain the secondary magnesium phosphate that organises;
(2) secondary magnesium phosphate that organises that α-cyanoacrylate and step (1) obtain is added in kneader and mediate 3 hours at 130 DEG C, be transferred in twin screw extruder and melt extrude 9 minutes, extrusion temperature is 170-210 DEG C, obtains base-material after cooling;
(3) base-material that step (2) obtains is added in stirring tank, stir and add aluminium hydroxide, pigment dyestuff, silica powder, liquid polyisobutene after 10 minutes, stir 2 hours at 100 DEG C, add PMMA, DOP after being cooled to room temperature, sulfurous gas, Resorcinol, cyanacrylate be stirred to and be uniformly dispersed, obtain α-cyanoacrylate heat-conducting glue.
After tested, impact resistance and the thermotolerance of embodiment 1-6 and comparative example are as shown in the table, wherein,
The Chinese patent of comparative example to be publication number be CN103484052B,
Shock-resistance is with reference to GB/T6328-1999, and by the shock strength of balance weight impact testing machine test sizing agent, shock strength shows that more greatly shock-resistance is better, and test condition is: steel-steel, shows speed 3.4m/s, test angle 150 degree, and probe temperature is 25 DEG C;
Thermotolerance adopts thermal analyzer to carry out thermogravimetric analysis to sizing agent and tests out heat decomposition temperature, and heat decomposition temperature is higher shows that thermotolerance is better, and test condition is: nitrogen atmosphere, and temperature rise rate 10 DEG C/min, rises to 600 DEG C from room temperature.
As seen from the above table, the shock strength of embodiment of the present invention 1-6, heat decomposition temperature, all higher than comparative example, show good shock-resistance and thermotolerance.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (10)
1. a α-cyanoacrylate heat-conducting glue, is characterized in that: by weight, is made up of following component: α-cyanoacrylate 100 parts, thickening material 2 ~ 5 parts, 2 ~ 4 parts, softening agent, stablizer 0.1 ~ 0.4 part, stopper 0.5 ~ 1 part, linking agent 20 ~ 30 parts, fire retardant 3 ~ 6 parts, pigment 1 ~ 2 part, heat conductive filler 100 ~ 110 parts, secondary magnesium phosphate 10 ~ 14 parts, liquid polyisobutene 8 ~ 10 parts.
2. a kind of α-cyanoacrylate heat-conducting glue according to claim 1, is characterized in that: described thickening material is PMMA.
3. a kind of α-cyanoacrylate heat-conducting glue according to claim 1, is characterized in that: described softening agent is DOP.
4. a kind of α-cyanoacrylate heat-conducting glue according to claim 1, is characterized in that: described stablizer is sulfurous gas.
5. a kind of α-cyanoacrylate heat-conducting glue according to claim 1, is characterized in that: described stopper is Resorcinol.
6. a kind of α-cyanoacrylate heat-conducting glue according to claim 1, is characterized in that: described linking agent is cyanacrylate.
7. a kind of α-cyanoacrylate heat-conducting glue according to claim 1, is characterized in that: described fire retardant is aluminium hydroxide.
8. a kind of α-cyanoacrylate heat-conducting glue according to claim 1, is characterized in that: described pigment is pigment dyestuff.
9. a kind of α-cyanoacrylate heat-conducting glue according to claim 1, is characterized in that: described heat conductive filler is aluminum oxide or silica powder.
10. the preparation method of a kind of α-cyanoacrylate heat-conducting glue according to claim 1 ~ 9 any one, is characterized in that: its step is as follows:
(1) secondary magnesium phosphate is added be uniformly dispersed in distilled water after obtain the secondary magnesium phosphate solution that massfraction is 10%, be that the octadecyl trimethyl ammonium chloride of secondary magnesium phosphate 1.8 times adds in secondary magnesium phosphate solution by weight, magnetic agitation 3 hours after microwave heating to 90 DEG C, dehydrated alcohol suction filtration is used after taking out, with distilled water wash 5 times, dry 4 hours at being placed in 90 DEG C, baking oven, after grinding, obtain the secondary magnesium phosphate that organises;
(2) secondary magnesium phosphate that organises that α-cyanoacrylate and step (1) obtain is added in kneader and mediate 3 hours at 130 DEG C, be transferred in twin screw extruder and melt extrude 9 minutes, extrusion temperature is 170-210 DEG C, obtains base-material after cooling;
(3) base-material that step (2) obtains is added in stirring tank, stir and add fire retardant, pigment, heat conductive filler, liquid polyisobutene after 10 minutes, stir 2 hours at 100 DEG C, add thickening material after being cooled to room temperature, softening agent, stablizer, stopper, linking agent be stirred to and be uniformly dispersed, obtain α-cyanoacrylate heat-conducting glue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510815239.9A CN105368330B (en) | 2015-11-23 | 2015-11-23 | A kind of a-cyanoacrylate heat-conducting glue and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510815239.9A CN105368330B (en) | 2015-11-23 | 2015-11-23 | A kind of a-cyanoacrylate heat-conducting glue and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105368330A true CN105368330A (en) | 2016-03-02 |
| CN105368330B CN105368330B (en) | 2018-11-27 |
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| CN201510815239.9A Active CN105368330B (en) | 2015-11-23 | 2015-11-23 | A kind of a-cyanoacrylate heat-conducting glue and preparation method thereof |
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| CN105950025A (en) * | 2016-05-22 | 2016-09-21 | 周淑华 | High-conductivity thermally conductive glue |
| CN105950024A (en) * | 2016-05-22 | 2016-09-21 | 周淑华 | Heat-conduction glue piece |
| CN106281059A (en) * | 2016-08-30 | 2017-01-04 | 盐城市艾斯特体育器材有限公司 | A kind of special adhesive of thermoplastic PVC table tennis |
| CN109233649A (en) * | 2018-09-17 | 2019-01-18 | 江苏创客新材料科技有限公司 | Viscous formula of a kind of binding dust paper roll height and preparation method thereof |
| CN110283538A (en) * | 2018-12-03 | 2019-09-27 | 上海康达化工新材料股份有限公司 | A kind of identifiable instant drying adhesive and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105950025A (en) * | 2016-05-22 | 2016-09-21 | 周淑华 | High-conductivity thermally conductive glue |
| CN105950024A (en) * | 2016-05-22 | 2016-09-21 | 周淑华 | Heat-conduction glue piece |
| CN106281059A (en) * | 2016-08-30 | 2017-01-04 | 盐城市艾斯特体育器材有限公司 | A kind of special adhesive of thermoplastic PVC table tennis |
| CN109233649A (en) * | 2018-09-17 | 2019-01-18 | 江苏创客新材料科技有限公司 | Viscous formula of a kind of binding dust paper roll height and preparation method thereof |
| CN110283538A (en) * | 2018-12-03 | 2019-09-27 | 上海康达化工新材料股份有限公司 | A kind of identifiable instant drying adhesive and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN105368330B (en) | 2018-11-27 |
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Denomination of invention: A type of alpha cyanoacrylate thermal conductive adhesive and its preparation method Granted publication date: 20181127 Pledgee: Agricultural Bank of China Limited Shaoxing Shangyu sub branch Pledgor: SHAOXING SHANGYU SHUNDONG RUBBER AND PLASTIC PRODUCT CO.,LTD. Registration number: Y2024980022234 |
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